离子色谱法同时测定高纯试剂中痕量甲胺、二甲胺、三甲胺和6种阳离子  

Simultaneous determination of trace monomethylamine, dimethylamine, trimethylamine and six cations in high purity reagents by ion chromatography

作　　者：罗全迁 霍世欣 LUO Quanqian;HUO Shixin(Metrohm China Limited,Shanghai 200335,China)

机构地区：[1]瑞士万通中国有限公司,上海200335

出　　处：《化学分析计量》2022年第3期48-52,共5页Chemical Analysis And Meterage

摘　　要：建立离子色谱法同时测定高纯试剂和有机溶剂中甲胺、二甲胺、三甲胺和6种阳离子的方法。对样品处理、色谱柱类型、淋洗液梯度等条件进行优化,实现了过氧化氢、乙醇、丙酮和异丙醇样品的直接进样分析。选用Metrosep C Supp 1阳离子交换柱进行梯度分离,采用微填充床阳离子抑制电导检测器检测。9种待测物质的质量浓度在5~200μg/L范围内与色谱峰面积具有良好的线性关系,相关系数均大于0.999,方法检出限为0.007~0.082μg/L。样品加标回收率为80.0%~110.5%,测定结果的相对标准偏差为0.58%~3.86%(n=5)。该方法满足高纯试剂中痕量有机胺杂质和阳离子的测定要求。A method for simultaneous determination of monomethylamine, dimethylamine, trimethylamine and six cations in high purity reagent and organic solvent by ion chromatography was established. The conditions of sample treatment, column type and eluent gradient were optimized to realize the direct injection analysis of hydrogen peroxide,ethanol, acetone and isopropanol samples. Metrosep C Supp 1 cation exchange column was selected for gradient separation,and micro packed bed cation suppression conductivity detector was used for detection. The mass concentration of the nine substances had a good linear relationship with the chromatographic peak area in the range of 5-200 μg/L, the correlation coefficients were all more than 0.999, and the detection limits of the method were 0.007-0.082 μg/L. The recoveries of spiked samples were 80.0%-110.5%, and the relative standard deviations of the determination results were 0.58%-3.86%(n=5). The method meets the requirements for the determination of trace organic amine impurities and cations in high purity reagents.

关 键 词：离子色谱法 微填充床阳离子抑制器 甲胺 二甲胺 三甲胺 高纯试剂 阳离子 

分 类 号：O657.7[理学—分析化学]